Патент USA US2114352код для вставки
April 19, 1938. Al A. vM11-1: l 2,114,352 PROCESS OF NEUTRALIZING HIGH BOILING PETROLEUM OILS Filed sept. 29, 1936 Patented Apr. 19, 1938 2,114,352 UNÍTED STATES PATENT OFFICE 2,114,352 PROCESS OF NEUTRALIZING HIGH BOIL'ING PETROLEUM OILS Arthur A. Neff, Paulsboro, N. J., assignor to `So-cony-Vacuum Oil Company, Incorporated, New York, N. Y., a corporation of New York Application September 29, 1936, Serial No. 103,066 2 Claims. (Cl. 196-1) This invention is directed to the reiining of figure of which sets forth the process in diagram oils, and particularly to the step of neutralizing matic form. In this drawing, the sour oil enters high boiling point oils which have been acid through pipe I into mixing tank 2 which serves as treated. an accumulator for the system. From tank 2 High boiling point petroleum fractions, of the the oil is forced by pump 3 through heat ex 5 nature of lubricating oils, transformer oils, and changer 4, where it is heated to 30D/350° F. and the like, are customarily refined by treatment then enters dry oil tank 5, which is equipped with with sulphuric acid, for the precipitation of as phaltic and color forming constituents, and the 10 like, resulting in the production of a sludge, which is settled and Withdrawn, to be discarded, and a so-called “sour” oil, which is neutralized and further reñned for the production of ñnished products. This invention has to do specifically 15 with this step of neutralization. There are two general methods of neutraliza tion practiced at present. The older method is by treatment with aqueous solutions of caustic soda. This may be, and usually is, preceded by 2 O a “gas blow”, in which the sour oil is thoroughly blown and agitated with air to remove, in so far as possible, all dissolved sulphur dioxide, and other oxides of sulphur which may be displaced during blowing. The sour oil at the end of the 25 “gas blow” is still high in acidity, and is then neutralized bytreatment with aqueous caustic soda. This operation is discontinuous, time con suming, and frequently encounters difliculties with emulsions, loss of oil color, and other trou 30 bles. A more modern method is one in which the sour oil is admixed with a small amount of al kaline absorbent clay, such as about 3-5% of fuller’s earth and the like, heated moderately, subjected to a “gas blow” operation at tempera 35 tures ranging from 200° F. to about 350° F., and the mixed slurry of oil and clay then heated to about 700° F., after which it is cooled and the oil and clay separated by filtration. This process a bottom steam spray 6 and a vent 1, in which is mounted a steam jet 8 to provide a moderate vacuum in tank 5. The hot oil is steamed thor 10 oughly in tank 5, under the vacuum existing therein, and is then withdrawn by pump 9 and passed through heat exchanger I0, being heated to about 400° F. and then passes through line Il and furnace heater I 2, where it is heated to a 15 temperature of G50/700° F. It is then discharged into foam tank I3, equipped with steam spray I4 and vent I5, where gases formed during the sec ond heating are expelled. The oil is then forced by pump I6 through pipe I1, heat exchangers I0 20 and 4, and pipe I8 into blending tank I9, where it is mixed with naphtha entering through pipe 20 in suflicient quantity to very materially reduce its viscosity. The solution from the blending tank is then strained to remove adventitious solid mat 25 ter and secure desired finish color by being forced by pump 2| through blotter press 22, after which it passes through percolation filter 23, (charged with absorbent clay), and is removed from the process as finished oil. With this process, with out the use of caustic and without contacting the sour oil with clay, it is quite possible to secure the same freedom from acidity as with former procedure. The blotter press and percolator, formerly charged with the duty of removing about 35 5% of fine clay from the oil, and constantly in diiiiculty, now only clarify the oil solution, and uses fine clay, and requires the use of filter remain on stream great periods of time without attention. Cost of clay consumed is completely 40 presses, thickeners, extractors, and the like for removal and recovery of the clay. Not only is there an added expense for clay purchase, but the operative steps of clay removal are frequently lessened. This capability of the process arises from its feature of heating in two stages, each followed in trouble, and give rise to high operative and 45 maintenance expense. The object of this invention is to provide a quick and eiiicient method for continuous neu tralization of sour oil which does not make use of admixed absorbent nor of caustic solutions. This invention is based upon the discovery that 50 complete neutralization may be attained by the application of heat and proper agitation with inert gas. In order to more completely under stand this invention, reference is made to the 55 drawing attached to this specification, the single 30 avoided, and operating attendance is greatly 40 by thorough agitation and sweeping with inert gas to remove the acidic constituents so set free. 45 In place of the steam, any inert gas, such as CO2, and the like may be used, although steam is to be preferred. The process may be carried out in other apparatus setups which will suggest them selves to the man skilled in the art as equivalents 50 of that which is herein disclosed by way of ex ample only and not for the purpose of limiting the disclosure thereby. I claim: 1. A process for completely neutralizing “sour” 55 2 2,114,352 acid-treated high-boiling petroleum fractions of from 300° to 350° F. in the absence of alkaline, Without the use of adsorptive, agglomerative, or adsorptive, or agglomerative material, thorough alkaline materials comprising the following steps: 1y steaming the oil so heated under a subatmos heating the oil to a temperature of from 300° to 350° F., and thoroughly agitating With inert gas while subjecting the oil to subatmospheric pres sure, thereafter further heating the oil to a. tem perature of from 650° to '700° F., and further thoroughly agitating with an inert gas. 2. A process for finishing “sour” acid-treated 10 high-boiling petroleum fractions comprising the following steps; heating the oil toa temperature pheric pressure, thereafter further heating ’the oil in the absence of alkaline, adsorptive, or ag 5 glomerative material to a temperature of from 650° to 750° F., thoroughly steaming the oil so heated, cooling the oil, adding thereto a Viscosity reducing diluent, subjecting diluted oil to a slight straining ñltration, and removing diluent. 10 ARTI-TUR A. NEFF.